DMA-80汞分析仪测定粗制氧化锌中的汞

doi:10.11962/1006-4990.2018-0497

Abstract

Abstract:

A method for the determination of mercury in crude zinc oxide by direct solid injection of DMA-80 mercury analyzer was established.The sample was dried and pyrolyzed,and the decomposition products were converted into oxidized mercury vapor by catalytic decomposition and adsorption purification,then reduced by the gold mercury singularity and captured in the form of gold amalgam,and finally the atomic absorption was measured at a wavelength of 253.65 nm,and quantified according to Lambert-Beer law.The experimental conditions such as drying time and temperature,decomposition time and temperature were optimized,and experiments such as detection limit,precision density and recovery rate were also carried out. Results showed that the detection limit of the method was 0.015 ng,the linear range was 0.02~100 ng,the correlation coefficient was≥0.999,the recovery rate was 93.2%~102.7%,and the precision（RSD,n=7）≤5.0%,which could be used for the rapid inspection of imported crude zinc oxide.

Key words: mercury analyzer, crude zinc oxide, mercury, pyrolysis, Beer law

CLC Number:

TQ132.41

Feng Junli,Yang Junfan,Wu Jingwu,Li Xu,Zhang Qingjian. Determination of mercury in crude zinc oxide by DMA-80 mercury analyzer[J]. Inorganic Chemicals Industry, 2019, 51(8): 73-75.

Figures/Tables 10

References 19

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汞含量/（μg·g^-1）	称样量/mg	汞含量/（μg·g^-1）	称样量/mg
100~200	0.5	2~20	5
50~100	1.0	0.02~2	10
20~50	2.0

水平	因素
水平	A 干燥时间/s	B 干燥温度/℃	C 分解温度/℃	D 分解时间/s
1	150	90	800	200
2	200	100	850	250
3	250	110	900	300

实验序号	因素水平				回收率/ %
实验序号	A	B	C	D	回收率/ %
1	1	1	1	1	97.76
2	1	2	2	2	98.68
3	1	3	3	3	98.32
4	2	1	2	3	98.92
5	2	2	3	1	98.05
6	2	3	1	2	97.83
7	3	1	3	2	98.13
8	3	2	1	3	97.99
9	3	3	2	1	99.25
k₁	98.253	98.270	97.860	98.353
k₂	98.267	98.240	98.950	98.213
k₃	98.457	98.467	98.167	98.410
R	0.203	0.227	1.090	0.197

坐标轴	标准点/ng	吸光度A	坐标轴	标准点/ng	吸光度A
长池工作线性范围	0	0.001 2	短池工作线性范围	0	0.015 3
	5	0.023 1		50	0.452 3
	20	0.085 2		100	0.881 6

水平/	测定值/ng							均数±标	RSD/	回收率/
（μg·g^-1）	1	2	3	4	5	6	7	准差	%	%
50	43.75	45.58	42.96	48.82	49.18	47.69	48.24	46.6±2.3	5	93.2
100	95.78	97.21	104.29	100.9	107.2	96.99	108.83	101.6±4.9	4.8	101.6
150	142.66	146.7	151.64	145.04	153.14	150.14	148.73	148.3±3.4	2.3	98.9
200	195.45	199.65	208.13	217.85	212.68	205.36	198.45	205.4±7.5	3.7	102.7

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

Determination of mercury in crude zinc oxide by DMA-80 mercury analyzer

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References 19

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样品编号	本法汞含量/	冷原子吸收光谱法
样品编号	（μg·g^-1）	汞含量/（μg·g^-1）
1-1523	0.086	0.077
1-2371	0.312	0.298

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